HJ 748-2015 English PDF

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HJ 748-2015: Water quality. Deterination of Thallium. Graphite furnace absorption Aectrophotometric method
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HJ 748-2015	229	Add to Cart	3 days	Water quality. Deterination of Thallium. Graphite furnace absorption Aectrophotometric method	Valid

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Basic data

Standard ID: HJ 748-2015 (HJ748-2015)
Description (Translated English): Water quality. Deterination of Thallium. Graphite furnace absorption Aectrophotometric method
Sector / Industry: Environmental Protection Industry Standard
Classification of Chinese Standard: Z16
Classification of International Standard: 13.060
Word Count Estimation: 9,925
Date of Issue: 2015-06-04
Date of Implementation: 2015-08-01
Quoted Standard: HJ/T 91; HJ/T 164; HJ 677; HJ 678
Regulation (derived from): Ministry of Environment Announcement 2015 No.43
Issuing agency(ies): Ministry of Ecology and Environment
Summary: This standard specifies the graphite furnace atomic Soluble thallium and thallium total absorption spectrophotometry. This standard applies to surface water, groundwater, sewage and industrial waste water was measured thallium. When precipitation enrichment method, sample enrichment to 50 times the method detection limit was 0.03��g/L, detection limit is 0.14��g/L. When direct measurement, detection limit is 0.83��g/L, detection limit was 3.3��g/L.

HJ 748-2015: Water quality. Deterination of Thallium. Graphite furnace absorption Aectrophotometric method

---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
Water quality.Deterination of Thallium.Graphite furnace absorption Aectrophotometric method Determination of thallium in water Graphite Furnace Atomic Absorption Spectrophotometry Water quality-Determination of Thallium-Graphite furnace absorption Apectrophotometric method 2015-06-23 released 2015-08-01 implementation National Environmental Protection Standard of the People 's Republic of China Ministry of Environmental Protection released Directory Preface ..ii 1 Scope of application 1 2 normative reference document 1 Principle of Method 1

4 interference and elimination

5 reagents and materials

6 instruments and equipment

7 samples

8 Analysis Step 4 The results are calculated and expressed 10 precision and accuracy 11 Quality assurance and quality control 12 Waste treatment 6

Foreword

In order to implement the Environmental Protection Law of the People's Republic of China and the Law of the People's Republic of China on the Prevention and Control of Water Pollution, the protection of the environment and the protection of the human body Safety and health, regulate the determination of thallium in water, the development of this standard. This standard specifies the thallium in water graphite furnace atomic absorption spectrophotometry. This standard is the first release. This standard is organized by the Ministry of Environmental Protection Science and Technology Standards Division. The main drafting unit of this standard. Shanghai Environmental Monitoring Center. The standard verification unit. the East China Sea Environmental Monitoring Center, Shanghai Metrology and Testing Technology Research Institute, Shanghai Xuhui District Environmental Monitoring Station, on Pudong New Area Environmental Monitoring Station, Shanghai Environmental Science Research Institute, Shanghai Textile Energy Conservation and Environmental Protection Center. The Environmental Protection Department of this standard approves on June 23,.2015. This standard is implemented from August 1,.2015. This standard is explained by the Ministry of Environmental Protection. Determination of thallium in water - Graphite furnace atomic absorption spectrophotometric method Warning thallium and thallium salts are highly toxic, thallium oxide and chloride have a certain volatility, the entire experimental process must be carried out in the fume hood.

1 Scope of application

This standard specifies the determination of soluble thallium and total thallium in water by graphite furnace atomic absorption spectrophotometry. This standard is applicable to the determination of thallium in surface water, groundwater, domestic sewage and industrial waste water. When the sample enrichment method was 50 times, the detection limit was 0.03 μg/L and the lower limit was 0.14 μg/L. When the direct determination, the detection limit of 0.83 μg/L, the determination of the lower limit of 3.3 μg/L.

2 normative reference documents

The contents of this standard refer to the following documents or their terms. For undated references, the valid version applies to this standard. Technical specification for surface water and wastewater monitoring Technical specification for groundwater monitoring of HJ/T 164 HJ 677 water quality of the total amount of metal digestion nitric acid digestion method Microwave digestion method for digestion of total water quality of HJ 678

3 Principle of the method

Precipitation enrichment method. in acidic conditions, with bromine as oxidant, the water thallium was trivalent state, with ammonia to adjust the pH, so that thallium in alkaline Conditions, and iron solution produced coprecipitation. Centrifugal separation of precipitation, and then dissolved in nitric acid solution precipitation, the treated sample into the graphite furnace atom In the vibrator, the thallium ions are atomized at high temperature in the graphite tube, and the characteristic lines of the thalium atoms in the ground state are selectively absorbed at 276.8 nm. The absorbance values Thallium concentration is proportional to. Direct method. the digestion of the pretreatment of the sample into the graphite furnace atomizer, the thallium ion in the graphite tube high temperature atomization, the ground state thallium atoms The absorbance of 276.8 nm characteristic lines is selectively absorbed, and the absorbance is proportional to the concentration of thallium.

4 interference and elimination

Chloride ion on the thallium negative interference, plus ammonium nitrate can effectively eliminate the concentration of less than 1.2 g/L of chloride ion interference. Sample storage, preparation and The preparation of standard solutions should avoid the use of hydrochloric acid.

5 reagents and materials

Unless otherwise stated, analytical analytical reagents conforming to national standards are used in the analysis, and the test water is freshly prepared deionized or distilled water. 25.1 concentrated nitric acid. ρ (HNO3) = 1.42 g/ml, excellent grade pure. 5.2 Nitric acid solution. 1 99. 5.3 Nitric acid solution. 1 1. 5.4 bromine water (Br2). 5.5 iron solution (Fe). ρ = 4 mg/ml. Weigh 14.28 g of ferric sulfate [Fe2 (SO4) 3] in 1000 ml of water. 5.6 Ammonia (NH3 • H2O). ω = 28%, ρ = 0.907 g/ml (20 ° C). 5.7 Ammonia (NH3 • H2O) solution. 1 9. 5.8 Mixed solution of palladium nitrate [Pd (NO3) 2] (0.3%)/magnesium nitrate [Mg (NO3) 2] (0.2%). Weigh 0.3 g of palladium nitrate, add 1 ml of concentrated nitric acid (5.1) dissolved. Weigh 0.2 g of magnesium nitrate dissolved in water. Mix the two solutions Water volume to 100 ml. 5.9 Ammonium nitrate (NH4NO3) solution. ω = 3%. Weigh 3.0 g of ammonium nitrate in 100 ml of water. 5.10 Thallium standard stock solution. ρ (Tl) = 1000 mg/L. Accurately weighed 1.3 g (accurate to 0.1 mg) about 105 ℃ drying 1 hour thallium nitrate (Tl NO3, excellent grade pure), add 50 ml Concentrated nitric acid (5.1), diluted with water to a volume of 1000 ml, shaken, stored in a polyethylene plastic bottle, or sold in a commercial Thallium standard solution. Standard stock solution can be stored for 12 months, commercially available thallium standard solution according to the manufacturer's storage time. 5.11 Thallium Standard Intermediate. ρ (Tl) = 50.0 mg/L. Remove the 5.00 ml thallium standard stock solution (5.10) in a 100 ml volumetric flask and dilute it with a nitric acid solution (5.2) and shake it. thallium Standard intermediate can be stored for 6 months. 5.12 Thallium standard use of liquid. ρ (Tl) = 1.00 mg/L. Remove 2.00 ml of thallium standard intermediate (5.11) in a 100 ml volumetric flask and dilute to the mark with nitric acid solution (5.2) and shake well. thallium Standard use of liquid can be stored for 6 months. 5.13 argon. purity not less than 99.99%.

6 instruments and equipment

Unless otherwise stated, the use of the national standard A-class glass gauge is used for the analysis. 6.1 Graphite Furnace Atomic Absorption Spectrophotometer. 36.2 Thallium hollow cathode lamp. 6.3 Magnetic stirrer. 6.4 centrifuge, with 50-100 ml centrifuge tube, the maximum speed. 4000 rpm (r/min). 6.5 microwave digestion device or electric plate. 6.6 Polyethylene bottles or hard glass bottles. 6.7 General laboratory equipment commonly used.

7 samples

7.1 Collection of samples Refer to HJ/T 91 Technical Specifications for Surface Water and Wastewater Monitoring and HJ/T 164 Technical Specifications for Groundwater Surveillance Water samples were collected and the sample collection was 1L. 7.2 Preservation of samples 7.2.1 soluble thallium samples The samples were collected and filtered through a 0.45 μm filter. The initial filtrate was discarded and the collected filtrate was stored in a polyethylene bottle or hard glass (6.6), every 100 ml of the filtrate plus 1 ml of concentrated nitric acid (5.1) acidified, measured within 14 days. 7.2.2 Total thallium samples Immediately after the collection of samples plus 10 ml of concentrated nitric acid (5.1) acidification, alkaline samples can increase the amount of acid. Samples are stored in a polyethylene bottle or hard Glass bottle (6.6), measured within 14 days. 7.3 Preparation of samples 7.3.1 Precipitation enrichment method Remove 500 ml or an appropriate amount of water in a 1000 ml beaker, acidify to pH = 2 with nitric acid solution (5.3), add 0.5 to 2 ml of bromine water (5.4) So that the water was yellow, 1 min does not fade prevail. Add 10 ml of iron solution (5.5), in the magnetic stirring, dropping ammonia (5.7), so that PH > 7, to be precipitated completely, carefully discard the supernatant, the sediment fraction into the centrifuge tube, centrifugal 15 ~ 20 min, remove the centrifuge tube, Absorb the supernatant with a straw. Add 1 ml of concentrated nitric acid (5.1) dissolved precipitation, transferred to 10 ml colorimetric tube, washed with water centrifuge tube, plus Into the 2 ml of palladium nitrate/magnesium nitrate mixed solution (5.8), if the chloride ion interference, plus 2 ml of ammonium nitrate solution (5.9), and finally with nitric acid Solution (5.2) diluted volume to the mark, mix, to be measured. 7.3.2 Direct method 4 sample digestion with reference to HJ 677-2013 or HJ 678-2013, add acid, placed in a microwave oven or electric plate digestion, sample digestion and evaporation To about 5ml. Cooling, filtering, adding 10ml of palladium nitrate/magnesium nitrate mixed solution (5.8), if the chloride ion interference, plus 10ml ammonium nitrate Solution (5.9), and finally with nitric acid solution (5.2) to 50ml. 7.3.3 blank samples Instead of the sample, the thallium blank sample was prepared according to the preparation procedure of the sample.

8 Analysis steps

8.1 Commissioning and calibration of instruments 8.1.1 Instrument reference conditions Refer to Table 1 for the instrumentation conditions. Each laboratory can choose the best measurement conditions according to the instrument manual. Table 1 Reference instrument determination conditions Measuring element Tl Light source Thallium hollow cathode lamp or special short arc hernia lamp Lamp current (mA) 7 Wavelength (nm) 276.8 Passband width (nm) 0.7 Drying temperature/time 80 ~ 120 ℃/30 s Ashing temperature/time 900 ℃/30 s Atomic temperature/time 1650 ° C/5 s Clear the temperature 2600 ℃/5 s Substrate modifier Pd (NO3) 2/Mg (NO3) 2 NH4NO3 Injection volume (μL) 20.0 Background deduction deuterium lantern background and Seaman buckle background 8.1.2 Drawing of calibration curves 8.1.2.1 Work curve drawing of precipitation enrichment method 5, respectively, to remove 0.00,0.50,1.00,1.50,2.00,2.50,5.00 ml Thallium standard use of liquid (5.12) in 50 ml volumetric flask, With nitric acid solution (5.2) constant volume to the line, shake. Standard series concentrations of 0.0,10.0,20.0,30.0,40.0,50.0,100.0 Μg/L. Respectively, to remove more than 10 ml standard series, in the 500 ml volumetric flask, diluted with water volume. According to (7.3.1) the preparation steps of the sample, Preparation of working curve series. 8.1.2.2 Standard curve drawing of direct method Respectively, to remove 0.00,0.50,1.00,1.50,2.00,2.50,5.00 ml Thallium standard use of liquid (5.12) in 50 ml volumetric flask, Add 10 ml of palladium nitrate/magnesium nitrate mixed solution (5.8), and 10 ml of ammonium nitrate solution (5.9), with nitric acid solution (5.2) Shake well The standard series concentrations were 0.0, 10.0, 20.0, 30.0, 40.0, 50.0 and 100.0 μg/L, respectively. The absorbance was measured by adding 20 μL of standard series to the graphite tube from the low concentration to the high concentration according to the selected optimum instrument conditions. To Absorbance for the vertical axis to thallium concentration (μg/L) as the abscissa, draw the calibration curve. 8.2 Determination of sample The absorbance of the sample was determined by the same conditions as the calibration curve. 8.3 blank experiment The absorbance of the thallium blank sample was measured according to the same conditions as the calibration curve.

9 Results calculation and representation

9.1 Results calculation The concentration of thallium in the sample ρ1 (μg/L) is calculated as follows. V12 -06  Where. ρ1 - the concentration of thallium in the sample, μg/L; Ρ2 - calibration curve in the test sample thallium concentration, μg/L; V - the volume of the sample taken, ml; V1 - the volume of the sample after preparation, ml. 9.2 The result is shown The results of the precipitation enrichment method retained two decimal places, and the results of the direct method retained three significant digits. 10 precision and accuracy 10.1 Precision 66 samples were used to measure simulated surface water samples with concentrations of 0.20 μg/L, 0.50 μg/L and 1.00 μg/L, respectively. The standard deviation was. 4.7% ~ 11%, 2.6% ~ 9.4%, 1.3% ~ 9.8%, respectively. The relative standard deviations were 19% 6.7%, 7.0%, the repeatability r was 0.038 μg/L, 0.084 μg/L, 0.15 μg/L, the reproducibility limit r was 0.10 μg/L, 0.12 μg/L, 0.23 μg/L. Six laboratories were tested for wastewater samples with concentrations of 36.0 μg/L and 87.0 μg/L, respectively. The relative standard deviations in the laboratory The relative standard deviations were. 4.4% and 5.2%, respectively. The reproducibility limit r was 2.2 μg/L, and the difference was between 0.85% and 3.4% 3.4 μg/L; reproducibility limit R was. 4.9 μg/L, 13 μg/L. 10.2 Accuracy 6 laboratories on the surface water samples were spiked, plus scalar were 0.10 μg, 0.25 μg, 0.50 μg, precipitation enrichment method plus standard The recoveries were 71% ~ 113%, 85% ~ 101%, 82% ~ 101%, respectively. The final recoveries were. 85% 32%, 93% 12%, 95% 13%. 6 laboratory for the concentration of 51.8 3 μg/L certified reference material by precipitation enrichment method for determination, the relative error. -5.6% ~ -1.4%; the relative error is. -4.1% 3.3%. 6 laboratories for the concentration of 36.0 μg/L of the waste water samples were spiked, plus scalar of 2.5 μg, the direct method of the spiked recovery rate 84% ~ 108%. The final recoveries of the direct method were 96% and 18%. 6 laboratories with a concentration of 51.8 3 μg/L of the certified reference material were measured by direct method, the relative error. -2.3% to 1.2%; The relative error is the final value. -0.5% 3.1%. 11 quality assurance and quality control 11.1 Each batch of samples should be blank test, the determination of the results below the detection limit. 11.2 each batch of samples should be 10% of the parallel sample analysis, parallel to the relative deviation should be controlled within 20%. 11.3 Each batch of samples should be 10% of the standard sample analysis, spike recovery should be controlled between 70% -120%. 11.4 The calibration curve should be plotted for each batch. In general, the correlation coefficient of the calibration curve should be above 0.995. Each measured 10 The sample should be measured to add an internal control sample or the middle of the working curve of the standard solution, the relative deviation of the measured results should be controlled within 10%, otherwise Redraw the calibration curve. 12 Waste treatment The waste generated in the experiment should be collected collectively in a covered container and clearly marked with a label, such as "toxic waste" Qualified units for processing. ......

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